钛取代杂多酸盐甘氨酸超分子化合物的合成及热分解动力学研究

Synthesis and non-isothermal kinetics of titanium substituted heteropolytungstates and glyine supermolecular compounds

用室温固相法合成了Keggin结构单取代杂多硅钨酸盐甘氨酸超分子化合物α-K4(HGly)3[SiW11Ti(H2O)O39].4H2O,用IR、UV、TG-DTA、X-射线粉末衍射等方法对其进行了表征。结果表明:甘氨酸阳离子与杂多阴离子主要靠静电作用结合,超分子化合物中杂多阴离子仍保持Keggin结构。同时,采用TG-DTA技术研究了标题化合物在氮气气氛中的热分解机理及非等温动力学,用Coats-Redfern的积分法和Achar的微商法对配合物的非等温动力学数据进行分析,得出了热分解反应的机理函数、动力学参数以及分解反应的活化能E和lnA。

Supermolecular compounds of glycine monosuhsti- tuted heteropolytungstates with Keggin structure α-K4 （ HGly） 3 [ SiW11 Ti （ H20 ） 039 ] · 4H2O were synthesized by solid phase reaction in room temperature. The structure was characterized by IR, UV, TG-DTA,X-ray diffraction. The results indicate that glycine combines the electrostatic effect with het- eropolytungstates. The heteropoly anion still remains its Keggin structure in supermolecular compounds. The non-isother- malkinetic data were analyzed with the used Coats-Redfern integral method and Achar differential method. The mechanism function, kinetic parameters, apparent activation energy E and pre-exponential factor InA of the thermal decomposition were obtained.